Manufacture of wooden stoppers.



No. 663,234. Patented nec. 4, |900. L. l.. LE FRANC. y

MANUFACTURE 0F WOODEN STOPPEBS.

(Application led Dec. 28; 1598.)

(no man.) Y a sheets-sheet 1.

Q c@ Q Q Nn. 663,234. Patented Dec. 4, |900. L. L. LE FRANC.

MANUFACTURE 0F WOODEN STDPPERS. (Application med me. 2s, leer.)

(No Model.) 3 Sheets-Sheet- 2.

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' N0`.sa3,'2s4. Ptented nec. 4, |900.

L. L. LE FRANC. 'MANUFACTURE 0F WOODEN STIOPPERS.

(Application led Dec. 28, 1898.)

`(Neu Model.) l3 Sheets-Sheet 3.

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UNITED STATES PATENT EFICEe Louis LEON LE FRANC, or Boso-LE-HARD,FRANCE.

MANUFACTURE Ol: WOODEN STOPPERS.

SPECIFICATION forming part of Letters Patent No. 663,234, dated December4, 1900.

Application filed December 28, 1898.

To a/ZZ whom it may concern:

Be it known that I, LoUIs LEON LE FRANC, a citizen of the Republic ofFrance, and a resident of Bosc-le-Hard, in the Republic of France, haveinvented a new and useful Im-` provement in the Manufacture of WoodenStoppers, which is fully set forth in the following specilication.

The experience gained in previous researches respecting the applicationof wood for corking liquids has convinced me that the methods which Ihave followed hitherto to render wood supple and impermeable presentedVdifficulties which rendered said system of corking too complicated. Itherefore began experiments with a View of avoiding said difficultiesand succeeded in doiugso by discovering a new method of treatment andpreparation of wood. These new methods govern my invention according tothe present application for patent.

In the treatment of wood for the purpose of rendering it supple I usedin the past acids for destroying to a certain extent the incrustatingsubstances'and the cellulose or alkaline solutions for eliminatingcompletely or partiallytheincrustatingsubstances. Ihave since found thatboth these means present a serious drawback. Both produce in the ber ofthe wood' such modications that the wood contracts when being dried,said contraction being sometimes very considerable.

A more thorough study of the wood fiber has convinced me that thechemical composition of theincrustating substances which give wood itsgreater or less strength is practically analogous to that of glucosidesand that cousequently said incrustatiug substances could be removed byoxidation. I therefore pursued my experiments as to treatment of wood inthis direction, and thus succeeded by oxidizing it in imparting to itremarkable qualities of suppleness by suitable elimination of theincrustating substance without rendering it liable to contraction orshrinkage.

The process of treatment of wood by oxidation maybe divided into twoprocessesone the treatment of hard wood-i. e., of wood with a largeproportion of incrustating matter-and the other of soft wood when suchis usedsuch as, for instance, poplar, in which the proportion ofincrustating matteris com- Serial No. 700,495. (No specimens.)

paratively small. However, by varying the strength of reagents usedeither of these processes may be used, whatever be the nature of thewood employed. In fact, the choice to be made is determined only byexperience. I may also oxidize the incrustatingsubstances by anywell-known oxidizing agents-metallic, alkaline, or earth-alkaline oxids,or peroxids, bichrornates, iodates, manganates, permanganates, sulfates,nitrates, chlorates, and alkaline or metal chlorids, or chromic, man`ganic, hydrochloric, chloro-chromic, nitric, duc., acids. All thesecompounds are employed at a strength determined by requirements. Inthese conditions it is possible to attain the desired results; but, asalready mentioned, I prefer to use one of the following methods,according to the particular case.

Processes of treating wood. First. For hard or semihard Wood or when anexceptional suppleness is to be obtained. In such cases I use nitricacid mixed with a chlorin derivative-such, for instance, as a solublechlorate. rlhis addition of chlorin not only has an oxidizing effect,but also prevent-s the wood from becoming colored by the treatment. Idilute the nitric acid mixed with an alkaline chlorate to an extentvarying with the nature of wood to be treated and determinedexperimentally, the point at which no more nitricacid fumes are formedbeing observed as a limit. As a rule 'the solution consists of onehundred parts of commercial nitric acid at 36o Baume and one hundredparts of water containing twenty parts of chlorate of potash or soda.The wood to be treated is placed in a closed vessel, constructed towithstand the action of the acid solution, either in blocks of across-section of, say, thirty millimeters square and of any length, orin the shape of cylinders or rods of the size of the coi-ks or Stoppers,or, which is preferable, in cylinders inwardly recessed, so as to reducethe proportion of liquid absorbed by the wood. When the receptacle isfilled with wood to about three-fourths of its volume, the acid solutionis introduced into it by suction. In order to accelerate the process ofimpregnation, the pressure in the apparatus is either reduced orincreased. The material remains in contact as long as necessary, theperiod of the treatment varying with the kind of wood IOO treated. It ispreferable to find the correct time experimentally; but as a generalrule the materials may remain in contact for from four to six hours at atemperature from 25 to 30 centigrade. When the oxidizing action hassufficiently modified the incrustating substances, the nitric solutionis drained 0E and immediately replaced by cold water. Lixiviation by acurrent of water is continued until the perfect neutrality is attainedand the last traces of the reagent have disappeared. This lixiviation isadvantageously assisted by an increase or reduction of pressure or bythe use of hot water toward the end of the operat ion. The solution usedfor the treatment may be employed again, provided that it is renewed orstrengthened as it becomes exhausted. The wood thus prepared isthoroughly dried and submitted to a process for rendering itimpermeable, which will be hereinafter described.

Second. Soft wood, more easy to render supple. In this case I preferablyemploy hydrochloric acid with an alkaline chlorate. This methodmay bealso, as already stated, applied to the treatment of hard wood, in whichcase it is simply necessary to use stronger solutions. In case of a softwood to be treated-"- such, for instance, as poplar-the process is asfollows: A solution of one hundred kilograms of water and [ive kilogramsof chlorate of potash or soda is prepared in an open leaden or evencopper vesselprovided with a heating device. The solution is boiled andthe wood is immersed as in the first case, preferably, however,in theshape of cylinders of the same size as the corks or, still better, inthe shape of such cylinders internally recessed for the purpose offacilitating subsequent lixiviation.' The whole is boiled 11ntil thewood is completely saturated with the chlorated water. When this pointis reached, a quantity Aof commercial hydrochloric acid equal to that ofthe alkaline chlorate is added to the vessel and the boiling continueduntil the alkaline chlorate is completely decomposed. This operation isslow, and it takes from three to four hours to arrive at a regularoxidation. The oxidation having thus been effected, the acid solution isdischarged and replaced by hot water, which is caused to circulate andis renewed until the reagents have been eliminated. Cold wat-er may alsobe used, in which case the wood is left in Vit for several days. Thiswood, freed from all foreign matter, is thoroughly dried and submittedto the operation for rendering it impermeable. A

Whichever of these methods be used whenever I proceed by oxidation Iobtain wood, which after being' immersed into hot, lukewarm, or coldwater becomes as supple and as elastic as cork.

I mentioned in the beginning of this description that the methodsaccording to which I operated to render wood impermeable and air andwater tight present certain difficulties esageriin the application tocorking with wood. In eect, owing to its texture, wood, unlike cork, canbe used for corking purposes only in the direction of its longitudinalfibers, as its transverse fibers are not strong enough. It follows that,owing to capillary action, it cannot be impermeable. In order to renderit impermeable, it is necessary to be able if not to stop or clog itslongitudinal texture throughout the whole of its length at least tointercept it to a sufficient extent to prevent the passage of liquids orgases. I found that if the introduction into the texture of wood ofasubstance which renders it impermeable is eected by the method I usedvbefore it is possible to render it impermeable; but then it presentsserious drawbacks from a practical point of view. In fact, if a stopperis immersed in a solution for rendering it imperineable and saidsolution is caused by pressure or vacuum to penetrate into its tissuesin all directionsthat is to say, both transversely and longitudinally ofthe fibersthe wood loses all its suppleness, becomes hard, rigid, andnearlyincompressible. Moreover, if by exercising a powerful pressure itis compressed so as to reduce its cross-section, which is oneof therequirements of corking, the

greater portion of the substance which renders itimpermeable willbepressed out. One is therefore face to face with the following drawbacks;The stopper having lost its elasticity requires a powerful pressure inorder to introduce it into the neck of the bottle, which it fits in avery imperfect manner owing to the same cause. The compression forcesout a portion of the substance, which, though it may be harmless,becomes mixed with the liquid in the bottle, and finally the expulsionof said substance from the liber removes the guarantee of impermeabilityof the stopper.

From the preceding and in order to allow of rsuccessful corking itfollows that the first thing to be obtained is the impermeability of thelong fiber, as it alone can let liquids or gases pass, the short ortransverse iibers not being able to let any liquid through, as theirends are effe'ctually closed by the contact with the neck of the bottle.This consideration underlies my new process, which is carried out in thefollowing manner: The stoppers having been rendered supple andlixiviated are dried to such an extent as to contain enough moisture toremain supple, or if it is desired to operate in a moreconstant mannerthey are thoroughly dried and afterward dipped into boiling water orsubmitted to the action of exhaust-steam until they have acquired thedesired elasticity. The Stoppers are then impregnated iu accordance withmy process, an apparatus such as shown in the drawings being employed.

In the drawings, Figure 1 is a plan view of a tray or plate on which theStoppers are placed, and Fig la is a longitudinal section thereof.portion is not completed, and it will be un- In both of these figuresthe central IOO IIO

derstood that it will appear like the end portions. Fig. 2 is atransverse section of the boiler or vessel in which the said trays orplates lled with stoppers are placed; and Fig. 3 is an end elevation ofthe same, partly broken away.

P indicates a plate or tray, which is provided with a large number ofholes t, arranged in parallel rows. The" holes if are slightly conicaland have a diameter at their upper part which is from two to fourmillimeters greater than that of the Stoppers, while at their lower partthey have a diameter at least a millimeter less. The thickness of thetray or plate is greater than the length of the Stoppers. The differencein diameter has for its object to produce a slight contraction of thestopper, so that it will snugly fit into the hole t. Only the upper andlower ends of the Stoppers will be in contact With the iinpregnatingsubstance, the sides being entirely inclosed. When the stoppers are tobe placed in position, they are softened by boiling water or steam andare then pressed into the holes t t by means of a machine similar tothat for coi-king bottles. When the plate or tray is filled withstoppers, vit is placed into a boiler or vessel I), which is ofcylindrical shape, of sheet metal, and is opened or closed by means of adoor n, which is sustained by a suitable support K. The vessel D isprovided with an interior heating-coil D or other suitable source ofheat, the temperature of which is regulated by a therinometer which islocated in one side of the vessel. Extending transversely across thevessel D is a series of shelves formed of bars R. Onto these shelves thetrays or plates illed with stoppers to be treated are placed. The vesselmay contain eleven to twelve trays or plates containing each threehundred stoppers, so that from three thousand three hundred to threethousand six hundred Stoppers can be treated at one operation.

For treating the Stoppers by means of paraflin, for example, theoperation is as follows: The vessel or boiler being hermetically closedis charged with trays or plates 'containing stoppers. Through a pipe C apartial vacuum is produced in the vessel by means of a suction-pump,while the liquid parain is drawn into the vessel through pipe A. Whenthe trays or plates are immersed in the parafn, the temperature israised to 80 or 90", while a Vacuum tension of from fifty-five to sixtycentimeters of mercury is produced, and under these conditions the wateris evaporated and is replaced by the paraiiin.

It is obvious that the evaporation of the water and the introduction ofthe paraftin can take place only through the upper and lower ends of thestoppers, as the cylindrical surfaces of the Stoppers are held underpressure throughout by the walls of the holes t t. Therefore theintroducing of the impregnating substance can only take place in thelongitudinal direction of the bers, which is essential, as has beenfully stated already. When the Stoppers have been fully impregnated,which is determined by practice, the vacu um is discontinued and the airpermitted to reenter through the pipe B and the paraffin permitted torun through pipe A into a suitable receptacle until it is again requiredfor use. The door n is then opened and the trays or plates containingthe Stoppers removed, so as to permit their gradual cooling. TheStoppers are afterward removed from the plates, which operation can bequickly effected by hand,although it is more convenient to do it bymeans of a machine somewhat similar to the one used for putting stoppersinto the plates.

For rendering the Stoppers impermeable I may use paraffin, stearine,wax, resins, gums, natural rubber, or rubber obtained from oils,gutta-percha, 85o., or a mixture of these substances. results: rubberfrom oil, twenty; colophony, thirty; stearine, ten; paraffin, forty.

By rubber or caoutchouc derived from oil is to be understood a substanceinvented by J. de Eilembourg in 1846 and which is obtained by boiling inwater, which is acidulated by nitric acid, the residuum which isobtained from oils subjected to a high tem-4 perature. The product is avery elastic body, soluble in ether, and can be obtained from theresiduum of nut and linseed oil.

I claim-- The process of treating wooden Stoppers, which consists insubjecting the wood of which the Stoppers are made to the action of aso- The following mixture gives good IOO lution of potassium chlorate,and afterward Louis LEON LE FRANC.

W'itnesses:

EDWARD P. MACLEAN, EMILE LEDREL.

IIO

